CN114525122A - Liquid carbon dioxide thickening agent and preparation method thereof - Google Patents
Liquid carbon dioxide thickening agent and preparation method thereof Download PDFInfo
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- CN114525122A CN114525122A CN202210189524.4A CN202210189524A CN114525122A CN 114525122 A CN114525122 A CN 114525122A CN 202210189524 A CN202210189524 A CN 202210189524A CN 114525122 A CN114525122 A CN 114525122A
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- C09K8/62—Compositions for forming crevices or fractures
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Abstract
The invention discloses a liquid carbon dioxide thickener and a preparation method thereof, aiming at the existing liquid CO2The invention combines the freeze-drying technology and successfully grafts the sulfydryl onto a long molecular chain by taking toluene as a solvent by using a solvothermal method so as to improve the oil displacement effect of the thickening agent and prepare the liquid CO with smaller friction coefficient and stronger sand-carrying capacity2The method has simple operation, low cost and repeatabilityGood performance and suitability for batch production.
Description
Technical Field
The invention belongs to the technical field of oil-gas field development, and relates to a liquid carbon dioxide thickening agent and a preparation method thereof.
Background
With the gradual reduction and exhaustion of conventional oil and gas resources, the efficient development of unconventional oil and gas is very important for guaranteeing the safety of energy strategies in China. In recent years, shale gas exploration and development are actively carried out in China, shale gas and coal bed gas are important components of unconventional natural gas, and a fracturing technology is a main yield increasing means for exploiting shale gas and coal bed gas at present. Wherein, in the fracturing design, the selection of the fracturing fluid has an important influence on the stimulation effect. At present, in the exploitation process of shale gas and coal bed gas, hydraulic fracturing fluid is used more generally in the fracturing technology, but the hydraulic fracturing technology not only has larger water consumption in the exploitation process, but also has unobvious transformation effect and pollutes the environment. In addition, the clay content of shale gas reservoirs in China is generally high, and clay minerals are easy to expand when meeting water, so that gas seepage channels are blocked and the reservoirs are damaged. Therefore, there is an urgent need to explore new technologies for developing unconventional resources. In recent years, supercritical carbon dioxide has become a hot point of research as a new fracturing medium. The supercritical carbon dioxide fluid replaces water to perform fracturing transformation on the shale gas reservoir and the coal bed, so that the anhydrous fracturing technology is realized, and the purposes of increasing yield and increasing permeability are achieved. In the process of reservoir fracturing operation, liquid carbon dioxide is used as sand carrying liquid to carry out yield increase operation, and besides cracks can be generated, the carbon dioxide can also greatly reduce the viscosity of crude oil. In the fracturing operation, liquid carbon dioxide is injected into a reservoir, and after the fracturing operation is finished, the carbon dioxide is quickly vaporized under the condition of the formation temperature and is mixed and dissolved in the formation crude oil, so that the viscosity of the crude oil can be greatly reduced. However,the problems of poor sand carrying capacity, large filtration loss of the carbon dioxide fracturing fluid and the like caused by low viscosity of the liquid carbon dioxide seriously influence the development of the carbon dioxide fracturing fluid to the direction of improving the recovery ratio. Thus, for existing liquid CO2The defects of poor fracturing and oil displacement effects and low burial viscosity are overcome, and the provision of the liquid carbon dioxide thickener and the preparation method thereof is particularly important. The invention combines the freeze-drying technology and utilizes a solvent method to successfully graft sulfydryl onto a long molecular chain by taking methylbenzene as a solvent, thereby successfully preparing the liquid CO with smaller friction coefficient and stronger sand-carrying capacity2A thickening agent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a liquid carbon dioxide thickener.
The invention is realized by the following steps:
a liquid carbon dioxide thickener and a preparation method thereof specifically comprise the following steps:
s1, dissolving macromolecules such as polyvinylpyrrolidone (PVP) or polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone, ultrasonic stirring for 15-25min, adding small amount of Al2O3Powder to ensure the smoothness;
s2, taking a proper amount of sulfur powder to dissolve in toluene, and adding 3-5ml of glycerol into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at high temperature, raising the temperature to 350 ℃ rapidly, keeping the temperature for 2-3h, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
Preferably, the macromolecular chain is polyvinylidene fluoride (PVDF)
Preferably, the time of the ultrasonic stirring is 18min
Preferably, the screw reaction kettle is a pressure-resistant and high-temperature-resistant 100ml stainless steel reaction kettle.
Compared with the prior art, the invention has the following beneficial effects:
1. the material prepared by the solvothermal method has low production cost, and the obtained thickening agent has good uniformity and strong repeatability.
2. The thickener prepared by the invention takes sulfur powder as an S source, and successfully adds the mercapto functional group on the long-chain macromolecule in a mode of dissolving S by toluene, thereby improving the thickening effect of the material.
3. The invention is modified based on the existing long-chain macromolecules, the used raw materials are common, the price is low, and the invention is suitable for industrial production.
4. Al is added in the preparation process of the thickening agent2O3And the friction force of the material is reduced.
Drawings
FIG. 1 is a high temperature, high pressure resistant 100ml screw reactor used in examples 1-4 of the present invention.
Fig. 2 is an XRD pattern of the thickener prepared in example 2 of the present invention.
Fig. 3 is an SEM magnified view of the material prepared in example 3 of the present invention.
Fig. 4 is an SEM image of the thickener prepared in example 4 of the present invention after lyophilization.
Detailed Description
Exemplary embodiments, features and performance aspects of the present invention will be described in detail below with reference to the accompanying drawings.
The invention provides a preparation method of a liquid carbon dioxide thickening agent, which specifically comprises the following steps:
s1, dissolving macromolecules such as polyvinylpyrrolidone (PVP) or polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone, ultrasonic stirring for 15-25min, adding small amount of Al2O3Powder to ensure the smoothness;
s2, taking a proper amount of sulfur powder to dissolve in toluene, and adding 3-5ml of glycerol into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at high temperature, raising the temperature to 350 ℃ rapidly, keeping the temperature for 2-3h, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
Example 1
S1, dissolving 10g of polyvinylpyrrolidone (PVP) macromolecules into 30ml of nitrogen methyl pyrrolidone, ultrasonically stirring for 15min, and adding a small amount of Al2O3Powder to ensure the smoothness;
s2, taking 1.8g of sulfur powder to dissolve into 30ml of toluene, and adding 3ml of glycerol into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at a high temperature, raising the temperature to 350 ℃ rapidly, keeping the temperature for 2 hours, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
FIG. 1 shows a high temperature and high pressure resistant 100ml screw reactor used in examples 1-4 of the present invention, which can be heated to 350 ℃ to ensure the safety of the experiment, and which can withstand higher temperatures without a polytetrafluoroethylene liner.
Example 2
S1, dissolving 15g of polyvinylidene fluoride (PVDF) macromolecules into 30ml of nitrogen methyl pyrrolidone, ultrasonically stirring for 25min, and adding a small amount of Al2O3Powder to ensure the smoothness;
s2, 2.5g of sulfur powder is taken and dissolved into 30ml of toluene, and 5ml of glycerol is added into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at a high temperature, rapidly raising the temperature to 350 ℃, keeping the temperature for 3 hours, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
FIG. 2 is an XRD pattern of the thickener prepared in example 2 of the present invention, from which it can be analyzed that the crystallinity of the material is good and Al is present2O3The frictional resistance of the thickener can be reduced.
Example 3
S1, dissolving 8g of polyvinylpyrrolidone (PVP) and 6g of polyvinylidene fluoride (PVDF) macromolecules into 30ml of nitrogen methyl pyrrolidone, ultrasonically stirring for 19min, and adding a small amount of Al2O3Powder to ensure the smoothness;
s2, dissolving 3g of sulfur powder into 30ml of toluene, and adding 4ml of glycerol into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at a high temperature, raising the temperature to 350 ℃ rapidly, keeping the temperature for 2.5 hours, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
FIG. 3 is an SEM magnified view of the material prepared in example 3 of the present invention, from which Al of the material can be seen2O3Small particles, indicating that the material is well mixed.
Example 4
S1, dissolving macromolecules such as 6g of polyvinylpyrrolidone (PVP) and 8g of polyvinylidene fluoride (PVDF) in 30ml of nitrogen methyl pyrrolidone, ultrasonically stirring for 17min, and adding a small amount of Al2O3Powder to ensure the smoothness;
s2, taking 2g of sulfur powder to dissolve in 30ml of toluene, and adding 4.3ml of glycerol into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at high temperature, raising the temperature to 350 ℃ rapidly, keeping the temperature for 2-3h, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
Fig. 4 is an SEM image of the thickener prepared in example 4 of the present invention after lyophilization, from which it can be seen that the material has a better hinge effect.
Finally, it should be noted that: the above-mentioned embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The invention provides a liquid carbon dioxide thickener and a preparation method thereof, which are characterized in that: the method specifically comprises the following steps:
s1, dissolving macromolecules such as polyvinylpyrrolidone (PVP) or polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone, ultrasonic stirring for 15-25min, adding small amount of Al2O3Powder to ensure the smoothness;
s2, taking a proper amount of sulfur powder to dissolve in toluene, and adding 3-5ml of glycerol into the solution to ensure that enough hydroxyl can grow on a macromolecular chain;
s3, mixing the other liquids prepared in the steps S1 and S2 uniformly, adding the mixture into a screw reaction kettle which can be used at high temperature, raising the temperature to 350 ℃ rapidly, keeping the temperature for 2-3h, and reacting sulfur powder with glycerol in the reaction kettle to generate sulfydryl;
s4, after the temperature of the reaction kettle is cooled, taking out a sample and freeze-drying the sample at-60 ℃;
and S5, grinding the freeze-dried colloid into powder to obtain the modified liquid carbon dioxide thickening agent.
2. The liquid carbon dioxide thickener and the preparation method thereof according to claim 1, wherein: the macromolecular chain in the S1 is polyvinylidene fluoride (PVDF).
3. The liquid carbon dioxide thickener and the preparation method thereof according to claim 1, wherein: the ultrasonic stirring time in the S1 is 18 min.
4. The liquid carbon dioxide thickener and the preparation method thereof according to claim 1, wherein: the screw reaction kettle is a pressure-resistant and high-temperature-resistant 100ml stainless steel reaction kettle.
5. The liquid carbon dioxide thickener and the preparation method thereof according to claim 2, wherein: the dosage of the N-methyl pyrrolidone in the S1 is 30 ml.
6. The liquid carbon dioxide thickener and the method for preparing the same according to claim 1 or 2, wherein: the amount of toluene used in S2 was 30 ml.
7. The liquid carbon dioxide thickener and the preparation method thereof according to claim 6, wherein: the amount of glycerol in the S2 is 4 ml.
8. The liquid carbon dioxide thickener and the preparation method thereof according to claim 7, wherein: the using amount of the macromolecular chain polyvinylidene fluoride (PVDF) in the S1 is 15 g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116478676A (en) * | 2023-03-08 | 2023-07-25 | 四川孔墨能源科技有限公司 | Efficient liquid carbon dioxide thickener and preparation process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116478676A (en) * | 2023-03-08 | 2023-07-25 | 四川孔墨能源科技有限公司 | Efficient liquid carbon dioxide thickener and preparation process thereof |
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